CN114773066A - Manufacturing method of toughened silicon carbide ceramic kiln furniture flat plate - Google Patents
Manufacturing method of toughened silicon carbide ceramic kiln furniture flat plate Download PDFInfo
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- CN114773066A CN114773066A CN202210556912.1A CN202210556912A CN114773066A CN 114773066 A CN114773066 A CN 114773066A CN 202210556912 A CN202210556912 A CN 202210556912A CN 114773066 A CN114773066 A CN 114773066A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 40
- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000000835 fiber Substances 0.000 claims abstract description 80
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 26
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 239000004917 carbon fiber Substances 0.000 claims abstract description 9
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 7
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 7
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000006229 carbon black Substances 0.000 claims abstract description 7
- 239000003365 glass fiber Substances 0.000 claims abstract description 7
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 75
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 17
- 238000001354 calcination Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 230000007774 longterm Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a method for manufacturing a toughened silicon carbide ceramic kiln furniture flat plate, which belongs to the technical field of ceramic kiln furniture and is characterized by comprising the following steps: the manufacturing method of the toughened silicon carbide ceramic kiln furniture flat plate comprises the following steps: adding silicon carbide powder, carbon black and boron carbide powder into ethanol, and performing ultrasonic treatment to form ethanol suspension; mixing alumina, magnesium fluoride and titanium alloy powder, and performing ball milling; mixing alumina whiskers and glass fibers to prepare a fiber filament 1, mixing the alumina whiskers and carbon fibers to prepare a fiber filament 2, transversely arranging the fiber filament 1, longitudinally arranging the fiber filament 2, and preparing the fiber filament 1 and the fiber filament 2 into a fiber net.
Description
Technical Field
The invention relates to the technical field of ceramic kiln furniture, in particular to a method for manufacturing a toughened silicon carbide ceramic kiln furniture flat plate.
Background
The kiln furniture is a high-grade refractory material, is a device made of refractory earth and has the functions of spacing, supporting, bearing, protecting and the like on a blank in the roasting process, and the quality of the kiln furniture is directly influenced by the quality of a sintered product and the production cost. With the rapid development of novel functional ceramics such as magnetic materials, electronic ceramics and the like, the requirements on the quality of kiln furniture are higher and higher, and the kiln furniture belongs to consumables, so that the kiln furniture material is required to have higher refractoriness, good thermal stability, higher normal temperature and high temperature strength, load of products and the kiln furniture, good thermal conductivity, low heat storage property, thermal shock resistance and oxidation resistance. Since the 80 s of the last century, the ceramic rapid sintering technology has been pursued at home and abroad, and silicon carbide ceramic has become the first material of high-temperature kiln furniture for rapid sintering kilns.
The silicon carbide ceramic material has the excellent characteristics of high-temperature strength, strong high-temperature oxidation resistance, good wear resistance, good thermal stability, small thermal expansion coefficient, large thermal conductivity, high hardness, thermal shock resistance, chemical corrosion resistance and the like, but the existing silicon carbide ceramic is brittle and easy to damage in the long-term use process.
Disclosure of Invention
The invention aims to provide a manufacturing method of a toughened silicon carbide ceramic kiln furniture flat plate, which aims to solve the problems that the existing silicon carbide ceramic proposed in the background art is brittle and easy to damage in a long-term use process.
In order to achieve the purpose, the invention provides the following technical scheme: a method for manufacturing a toughened silicon carbide ceramic kiln furniture flat plate is characterized by comprising the following steps: the manufacturing method of the toughened silicon carbide ceramic kiln furniture flat plate comprises the following steps:
s1: adding silicon carbide powder, carbon black and boron carbide powder into ethanol, and performing ultrasonic treatment to form ethanol suspension;
s2: mixing aluminum oxide, magnesium fluoride and titanium alloy powder, and performing ball milling to obtain metal powder;
s3: mixing the alumina whiskers and the glass fibers to prepare a fiber filament 1, mixing the alumina whiskers and the carbon fibers to prepare a fiber filament 2, transversely arranging the fiber filament 1, longitudinally arranging the fiber filament 2, and preparing the fiber filament 1 and the fiber filament 2 into a fiber net;
s4: putting the metal powder obtained in the step S2 into the ethanol suspension obtained in the step S1, grinding and mixing to obtain slurry;
s5: putting the slurry into a mold, placing the fiber net on the top of the slurry, putting the slurry again, overlapping the slurry and the fiber net with each other, and filling the slurry and the fiber net in an inner cavity of the mold until the mold is filled with the slurry, and vibrating the slurry through a vibrating device to uniformly fill the slurry in the inner cavity of the mold;
s6: placing the mould filled with the slurry into a drying device for drying until the slurry is in a semi-dry state;
s7: placing a counterweight in the inner cavity of the mold to contact with the semi-dry slurry, applying gravity to the slurry through the counterweight, heating, and filling inert gas for constant-temperature sintering for 2.5-4 h;
s8: cooling to 500-600 ℃ at the cooling rate of 50-70 ℃/min, calcining for 1-3h, then heating to 1300-1400 ℃ at the heating rate of 200-250 ℃/min, calcining for 1-2h, keeping the temperature for 1-2h, and finally cooling to room temperature at the cooling rate of 100-150 ℃/min to obtain the silicon carbide ceramic kiln furniture plate.
Preferably, the ethanol addition volume in the step S1 is 200-500 times of the volume of the silicon carbide micropowder.
Preferably, the ball milling time in the step S2 is 1-2 h.
Preferably, the drying temperature in the step S6 is 50 to 75 ℃.
Preferably, the heating at temperature rising in the step S7 is performed at a heating rate of 70-90 ℃/min to 1400-1600 ℃.
Compared with the prior art, the invention has the beneficial effects that: according to the manufacturing method of the toughened silicon carbide ceramic kiln furniture flat plate, the alumina whiskers and the carbon fibers are mixed to form the fiber filaments 2, the fiber filaments 1 are transversely arranged, the fiber filaments 2 are longitudinally arranged, the fiber filaments 1 and the fiber filaments 2 are made into fiber nets, the fiber nets are added to the prepared silicon carbide ceramic kiln furniture flat plate, and the toughness of the prepared silicon carbide ceramic kiln furniture flat plate is enhanced through the fiber nets.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for manufacturing a toughened silicon carbide ceramic kiln furniture flat plate, which comprises the following steps of mixing alumina whiskers and carbon fibers to prepare fiber filaments 2, transversely arranging the fiber filaments 1, longitudinally arranging the fiber filaments 2, preparing the fiber filaments 1 and the fiber filaments 2 into fiber nets, adding the fiber nets into the prepared silicon carbide ceramic kiln furniture flat plate, and reinforcing the fiber nets to obtain the toughness of the toughened silicon carbide ceramic kiln furniture flat plate, wherein the method for manufacturing the toughened silicon carbide ceramic kiln furniture flat plate comprises the following steps:
s1: adding silicon carbide powder, carbon black and boron carbide powder into ethanol, and performing ultrasonic treatment, wherein the volume of the ethanol is 500 times that of the silicon carbide micropowder, so as to form ethanol suspension;
s2: mixing aluminum oxide, magnesium fluoride and titanium alloy powder, performing ball milling for 1-2h to obtain metal powder;
s3: mixing the alumina whiskers and the glass fibers to prepare a fiber filament 1, mixing the alumina whiskers and the carbon fibers to prepare a fiber filament 2, transversely arranging the fiber filament 1, longitudinally arranging the fiber filament 2, and preparing the fiber filament 1 and the fiber filament 2 into a fiber net;
s4: grinding and mixing the metal powder obtained in the step S2 in the ethanol suspension obtained in the step S1 to obtain slurry;
s5: putting the slurry into a mold, placing the fiber net on the top of the slurry, putting the slurry again, overlapping the slurry and the fiber net to fill the inner cavity of the mold until the slurry fills the mold, and vibrating the slurry through a vibrating device to uniformly fill the slurry into the inner cavity of the mold;
s6: placing the mould filled with the slurry into a drying device for drying at the drying temperature of 50-75 ℃ until the slurry is in a semi-dry state;
s7: placing a counterweight in the inner cavity of the mold to be contacted with the semi-dry slurry, applying gravity to the slurry through the counterweight, heating to 1400-1600 ℃ at the heating rate of 70-90 ℃/min, filling inert gas for constant-temperature sintering for 2.5-4 h;
s8: cooling to 500-600 ℃ at the cooling rate of 50-70 ℃/min, calcining for 1-3h, then heating to 1300-1400 ℃ at the heating rate of 200-250 ℃/min, calcining for 1-2h, keeping the temperature for 1-2h, and finally cooling to room temperature at the cooling rate of 100-150 ℃/min, thus obtaining the toughened silicon carbide ceramic.
Example 1
The manufacturing method of the toughened silicon carbide ceramic kiln furniture flat plate comprises the following steps:
s1: adding silicon carbide powder, carbon black and boron carbide powder into ethanol for ultrasonic treatment, wherein the volume of the ethanol added is 300 times of that of the silicon carbide micropowder, so as to form ethanol suspension;
s2: mixing aluminum oxide, magnesium fluoride and titanium alloy powder, performing ball milling for 1-2h to obtain metal powder;
s3: mixing alumina whiskers and glass fibers to prepare a fiber filament 1, mixing the alumina whiskers and carbon fibers to prepare a fiber filament 2, transversely arranging the fiber filament 1, longitudinally arranging the fiber filament 2, and preparing the fiber filament 1 and the fiber filament 2 into a fiber net;
s4: putting the metal powder obtained in the step S2 into the ethanol suspension obtained in the step S1, grinding and mixing to obtain slurry;
s5: putting the slurry into a mold, placing the fiber net on the top of the slurry, putting the slurry again, overlapping the slurry and the fiber net with each other, and filling the slurry and the fiber net in an inner cavity of the mold until the mold is filled with the slurry, and vibrating the slurry through a vibrating device to uniformly fill the slurry in the inner cavity of the mold;
s6: placing the mould filled with the slurry into a drying device for drying at the drying temperature of 60 ℃ until the slurry is in a semi-dry state;
s7: placing a counterweight in the inner cavity of the mold to be in contact with the semi-dry slurry, applying gravity to the slurry through the counterweight, heating to 1500 ℃ at the heating rate of 70 ℃/min, and filling inert gas for constant-temperature sintering for 3 hours;
s8: cooling to 550 ℃ at a cooling rate of 60 ℃/min, calcining for 1.5h, heating to 1370 ℃ at a heating rate of 200 ℃/min, calcining for 1.4h, preserving heat for 1.h, and finally cooling to room temperature at a cooling rate of 130 ℃/min to obtain the toughened silicon carbide ceramic.
Example 2
The manufacturing method of the toughened silicon carbide ceramic kiln furniture flat plate comprises the following steps:
s1: adding silicon carbide powder, carbon black and boron carbide powder into ethanol, and performing ultrasonic treatment, wherein the volume of the ethanol is 400 times of that of the silicon carbide micropowder to form ethanol suspension;
s2: mixing alumina, magnesium fluoride and titanium alloy powder, and performing ball milling for 1.7 hours to prepare metal powder;
s3: mixing the alumina whiskers and the glass fibers to prepare a fiber filament 1, mixing the alumina whiskers and the carbon fibers to prepare a fiber filament 2, transversely arranging the fiber filament 1, longitudinally arranging the fiber filament 2, and preparing the fiber filament 1 and the fiber filament 2 into a fiber net;
s4: grinding and mixing the metal powder obtained in the step S2 in the ethanol suspension obtained in the step S1 to obtain slurry;
s5: putting the slurry into a mold, placing the fiber net on the top of the slurry, putting the slurry again, overlapping the slurry and the fiber net to fill the inner cavity of the mold until the slurry fills the mold, and vibrating the slurry through a vibrating device to uniformly fill the slurry into the inner cavity of the mold;
s6: placing the mould filled with the slurry into a drying device for drying at 55 ℃ until the slurry is in a semi-dry state;
s7: placing a counterweight in the inner cavity of the mold to contact with the semi-dry slurry, applying gravity to the slurry through the counterweight, heating to 1550 ℃ at a heating rate of 75 ℃/min, and filling inert gas for constant-temperature sintering for 2.9 h;
s8: cooling to 530 ℃ at a cooling rate of 57 ℃/min, calcining for 2h, heating to 1370 ℃ at a heating rate of 240 ℃/min, calcining for 1.5h, preserving heat for 1.7h, and finally cooling to room temperature at a cooling rate of 140 ℃/min to obtain the toughened silicon carbide ceramic.
Example 3
The manufacturing method of the toughened silicon carbide ceramic kiln furniture flat plate comprises the following steps:
s1: adding silicon carbide powder, carbon black and boron carbide powder into ethanol for ultrasonic treatment, wherein the volume of the ethanol added is 450 times of that of the silicon carbide micropowder, so as to form ethanol suspension;
s2: mixing aluminum oxide, magnesium fluoride and titanium alloy powder, carrying out ball milling for 1.3h to obtain metal powder;
s3: mixing alumina whiskers and glass fibers to prepare a fiber filament 1, mixing the alumina whiskers and carbon fibers to prepare a fiber filament 2, transversely arranging the fiber filament 1, longitudinally arranging the fiber filament 2, and preparing the fiber filament 1 and the fiber filament 2 into a fiber net;
s4: grinding and mixing the metal powder obtained in the step S2 in the ethanol suspension obtained in the step S1 to obtain slurry;
s5: putting the slurry into a mold, placing the fiber net on the top of the slurry, putting the slurry again, overlapping the slurry and the fiber net with each other, and filling the slurry and the fiber net in an inner cavity of the mold until the mold is filled with the slurry, and vibrating the slurry through a vibrating device to uniformly fill the slurry in the inner cavity of the mold;
s6: placing the mould filled with the slurry into a drying device for drying at the drying temperature of 70 ℃ until the slurry is in a semi-dry state;
s7: placing a counterweight in the inner cavity of the mold to contact with the semi-dry slurry, applying gravity to the slurry through the counterweight, heating to 1500 ℃ at a heating rate of 80 ℃/min, and filling inert gas for constant-temperature sintering for 3 h;
s8: cooling to 580 ℃ at a cooling rate of 60 ℃/min, calcining for 2h, then heating to 1340 ℃ at a heating rate of 225 ℃/min, calcining for 2h, keeping the temperature for 1.7h, and finally cooling to room temperature at a cooling rate of 145 ℃/min to obtain the toughened silicon carbide ceramic.
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the disclosed embodiments of this invention can be used in any combination with one another as long as no structural conflict exists, and the combination is not exhaustively described in this specification merely for the sake of brevity and resource savings. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (5)
1. A method for manufacturing a toughened silicon carbide ceramic kiln furniture flat plate is characterized by comprising the following steps: the manufacturing method of the toughened silicon carbide ceramic kiln furniture flat plate comprises the following steps:
s1: adding silicon carbide powder, carbon black and boron carbide powder into ethanol, and performing ultrasonic treatment to form ethanol suspension;
s2: mixing alumina, magnesium fluoride and titanium alloy powder, and performing ball milling to obtain metal powder;
s3: mixing the alumina whiskers and the glass fibers to prepare a fiber filament 1, mixing the alumina whiskers and the carbon fibers to prepare a fiber filament 2, transversely arranging the fiber filament 1, longitudinally arranging the fiber filament 2, and preparing the fiber filament 1 and the fiber filament 2 into a fiber net;
s4: grinding and mixing the metal powder obtained in the step S2 in the ethanol suspension obtained in the step S1 to obtain slurry;
s5: putting the slurry into a mold, placing the fiber net on the top of the slurry, putting the slurry again, overlapping the slurry and the fiber net to fill the inner cavity of the mold until the slurry fills the mold, and vibrating the slurry through a vibrating device to uniformly fill the slurry into the inner cavity of the mold;
s6: placing the mould filled with the slurry into a drying device for drying until the slurry is in a semi-dry state;
s7: placing a counterweight in the inner cavity of the mold to contact with the semi-dry slurry, applying gravity to the slurry through the counterweight, heating, and filling inert gas for constant-temperature sintering for 2.5-4 h;
s8: cooling to 500-600 ℃ at the cooling rate of 50-70 ℃/min, calcining for 1-3h, then heating to 1300-1400 ℃ at the heating rate of 200-250 ℃/min, calcining for 1-2h, keeping the temperature for 1-2h, and finally cooling to room temperature at the cooling rate of 100-150 ℃/min to obtain the silicon carbide ceramic kiln furniture flat plate.
2. The method for manufacturing the toughened silicon carbide ceramic kiln furniture flat plate as claimed in claim 1, wherein the method comprises the following steps: the ethanol addition volume in the step S1 is 200-500 times of the volume of the silicon carbide micropowder.
3. The method for manufacturing the toughened silicon carbide ceramic kiln furniture flat plate as claimed in claim 2, wherein the method comprises the following steps: the ball milling time in the step S2 is 1-2 h.
4. The method for manufacturing the toughened silicon carbide ceramic kiln furniture flat plate as claimed in claim 3, wherein the method comprises the following steps: the drying temperature in the step S6 is 50 to 75 ℃.
5. The method for manufacturing the toughened silicon carbide ceramic kiln furniture flat plate as claimed in claim 4, wherein the method comprises the following steps: the heating in step S7 is heating to 1400-1600 ℃ at a heating rate of 70-90 ℃/min.
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CN116462525A (en) * | 2023-06-19 | 2023-07-21 | 中国人民解放军国防科技大学 | Continuous carbon fiber reinforced ultrahigh-temperature ceramic matrix composite material and preparation method thereof |
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